Apparatus for the distillation of solid materials



c. P. TOLMAN 1,773,893

APPARATUS FOR THE DISTILLATION OF SOLID MATERIALS Filed June 3, 1925 5 Sheets-Sheet l Aug. `26, 1930.

K. WQ A RM. A

I TroR'NEy.

A INVENTOR.

Qmhm@ 55km. KWK NQ KS* @HHH uw ,MN im@ u $5.9@ 2G N l Aug. 26, l930.- c. P. TOLMAN APPARATUS FOR THE DISTILJATION OF SOLID MATERIALS y 5 Sheets-Sheet 2 Filed June 3! 1925 INVENTOR. @www 7M B Y Aug.26,193o.` P TLNUWv 1,773,893

APPARATUS FOR THE DISTILLATION OF SOLID MATERIALS Find Jun 3, 1925` 5 sheets-sheet s fici/vif? ,waz

IN VEN TOI?.

ATTORNEY. P:

CHARLES P. 'TOLIAIL f shale, coal, lignite and similar materials,

Patented Aug. 26, 1930 UNITED sTATEs PATENT OFFICE OF KEW GARDENS, NEW YORK, ASSIGNOB, BY MESNE ASSIGN- MENTS, TO PETROLEUM CONVERSION CORPORATION, F NEW YORK, N. Y.

APPARATUS FOR THE DISTILLATION OI SOLID MATERIALS Application illed June 'S 1.925. Serial No. 34,544.

I roved form of apparatus suitable for the neat treatment or so-called distillation of carbonaceous materials,such for example, as il y 1 means of heated hydrocarbon gases or gases able for carrying view, partly in section` vzo heating elements ma derived therefrom. Such apparatus, however, is of utility for the stated purpose irrespective of the particular composition of the heat carrier gas used.

In the accompanying drawings, I have shown an improved form of apparatus suitout my improved process. Figure 1 is an elevational of one arrangement of apparatus; Fig. 2 is a lan view of the apparatus shown in Fig. 1; ig. 2'L is a cross section through one' of the blast stoves taken on line a-a of Fig. 1; and Fig. 3 is an elevational view of a modified form of apparatus.

Briefly stated the apparatus consists of a regenerative heating e ement or other source In said drawings,

of hydrocarbon gases heated to the requisitev temperature, a suitable distillation chamber, suitable condensing means and preferably a holder or reservoir for 'the gases utilized in the system.l Means are also provided for ac 'complishing purging of the systemfat suitable points. The heating elements which I prefer to use are hot blast stoves of the type similar to those used in the blast furnace art, although itis tobe understood that other types of gas be used. Referring particu arly to Figs. 1 and 2, 10 denotesone of a plurality of hot blast stoves. These stoves are identical in constructionso that a description of one will suffice for -all of them.l Stove 10 has a central duct 11 around which isarranged suitable checkerwork 12 so as to provide a plurality of vertical passages or flues. The stove 1s heated by means 'o one or more burners 13 at the bottom1 thereof the productsy of combustion passing upwardly t rough duct 11 and downwardl throu h checkerwork 12, and are vente throng pipe' 14 (see Fig. 2*). The

and the heat-ed gases.

.v spectively,

as to be heated enters through valved pipe l and le aves the stove through valved pipe 16.

The hot gases from one of the blast stoves v are introduced into distillation chamber 2O through pipe 16. Previously the chamber 20 has been filled with the material undergoing hea-t treatment e. g., ground to a suitable degree of fineness. The vapors generated by the heating are led from chamber 20. through valved p1pe 33 to condenser 22, the condensate therefrom collecting in receiver 23. 'I he gases and uncondensed vapors from the condenser 22 are drawn through and are a ain' ed to the stove 10 .which is being use for heating. A connection from receiver 23 to a as receiver 26 is provided in tl'ie form of a p1pe v27 provided with a relief valve 28, which is set to be operative when the pressure exceeds a predetermined value.

The construction of chamber 20 is apparent from Fig. 1. As shown, means are provided in the form of baflles 30, for insuring intimate contact between the more or less finely divided material undergoing heat treatment In the illustrative a plurality of distillation chamber designated 20, 2O"L and 2Ob order that the chamber 20, for example, may be charged while chamber 20 is running, whereas chamber 20b may be discharged during the same operation. To insure continuous operation, three-hot blast stoves, 10, and 10" are provided., each of the stoves being joined to its respective distillation chamber by f valved conduits 16, 16, and'16". Chambers 20, and 20b are, in turn, joined toa main 31 through valved pipes 32, 32 and 32", re-

each oft ese pipes having a valve, asfx shown. Main 31fis connected with condenser 22 by means of pipe 33, and thus any one of the three distillation chambers 20, 20 and-20b may be placed in communication with condenser 22 to the exclusion of the other two. Means are provided for purging the stoves and the distillation chambers. Steam main 35 .is provided with a branch 36 connectin stoves 10, 10 and 10"- andlpwith a branch 3 connecting each of distillation chambers-20,

oil-shale which has been form of Figs. 1 and 2,

are preferably provided in 20El and 201. The purge from the stoves may be removed either through main 38 or throughchimney conduits 14, while that from the distillation chambers is taken ofil through main'39, both main 38 and 39 joining a conduit 40 leading to receiver 26. The valve connections from steam branch 36, I deignate as 41, 41 and 41, respectively, and the oi'takes from the stoves to purge main 38 as 42, 42L and 42h, respectively. Similarly, 43, 43*I and 43b designate the valved connections from steam branch 37 to the distillation chambers, while 44, 44a and 44h indicate the offtake connections from the chambers to 'purge branch 39. Similar parallel connections are provided for the return pipe 24 returning gas to the stoves, these connectionsv being valved and designated 15, and l5".

To explain the operation of the apparatus, let it be assumed that the plant has not been operated and is about to be set in operation.

.It may be assumed that distillation chamber has been charged andthat the stove 10 is about to `be brought up to temperature.n

Thisl being the initial operation, it will be necessary to purge the bulk of the air from the system. Accordingly, the connection 41 ture by bustion being accumulated in the brick checkto steam line 36 is opened, and the appropriate valved connections manipulated `so as to connect stove 10, chamber 20, condenser 22, receiver 23, valves 46 and 47 being opened.l

When the system has been adequately purged by this through-.flow of steam, valves 46 and 47 are closed, aswell as connection 41,,admitting steam to the stove 10. It will be noted that in the subsequent operation purging will be done through valved connec- .tion 42, main 38 and conduit 40 to receiver 26 when gas is purged from the chamber. When air is purged from the stove 1Q, it is vented through a valve 140 in chimney conduit 14,

4 'Ihe stove is now broughtup to temperameansof burner 13, the heat of comerwork of the stove. In the meantime, stoves l()l and 10h have been similarly purged and charged with the material to source Joined by valved connection 47 or by admitting a hydrocarbon material to the pipe 18 as described below. The materiatis fed.

in' until the gaseous products formed by the -posited therein.

' evolution of flow into condenser 22. The temperature of the gas may be suitably regulated by means of a valved by-pass joining branch gas conduit 15 with gas conduit 16,-not shown. Upon leaving the condenser, the liquid fractions are accumulated in receiving tank 23 and the gas,

now cooled from its passage through the condenser, 'lows through pipe 24 to pump 25, whereby continuous circulation is maintained.

The pressure in the system can be increasedas desired by admitting to the stove hydrocarbon materials such for example as the heavy oils which break down into gases and light vapors upon their coming into contact with the heated checker Work of such stove," due attention being given relief valve 28 in conduit 27. vAs the operation proceeds, the store of heat in the stove 10 is progressively exhausted. Preferably the capacity of each stove is so chosen that the heat stored in stove 10, for example, will be reduced to an operating minimum when the treatment of charge in chamber 20 is completed. The available heat in stove 10 having been exhausted, stove 10a, which in the meantime has been heated,

purged and charged with gas to the pressure is connected in circuit with by opening valved connections 15'l and 16a. The stove 10 is then'cut out of the circuit and it and chamberl 20 are purged of their contained gas by establishing through valved connection ,44, communication with .pipes 39 and 40 leading to receiver of the system, chamber 20a 25 and then toward the end of the operation,

opening steam valved connection 41. In this manner the tion, is saved. Stove 1() is now cut off from chamber 20, the 'chimney valve opened and reheating of the stove begun by starting burnerf.

In the meantime, if treatment of the charge has been completed at the end of the cycle, the treated material is discharged from distillingchamber 20 and a fresh charge de- Preferably the valves in connections 32, as wellas valves 32l and 32h between the distilling chambers 2Oy and the main 31 are of the non-'returntype,permitting flow from the retort Ato the condenser, but not in the, reverse' direction. Therefore, such gas or vapor as may take place in virtue of the residual heat pass freely to the condenser if in the retort thereof, may

such accumulation builds to a pressure in eX-' cess of the pressure 'of the system.

In this manner the various distilling chambers are successively charged and discharged and the Acorresponding hot v blast stoves brought up to temperature cut in'and cut out gas contained in the stove and .,distilling chamber at the end ofthe opera- Y Assuming the system to be in whereby the system is made practically conconduction of heat tinuous.

In'Fig. 3, I have illustrated -a system wherein the distillation chambers may be dis- .without interrupting charged and charged operation. c As'shown, a distillingvchamber 200 is' provided having in valved communication therewith a charging hopper 200 and a discharging hopper 200", both of approxi mately the same capacity as chamber 200.` A stove 100 supplies hot hydrocarbon gases through pipe 101 to chamber 200, the prodi ucts therefrom `passing to a condenser 202, communicating with which is a receiver 203. A steam pipe 204 supplies steam `for purging to the bottom of chambers 200, 200e and 200". operation, and itis desiredto remove treated'material from chamber 200 (hopper 200b being empty) the pressure between the hoppers 200 and 200b is first equalized by admitting cold. gas through valved connection 205 into hopper 200", whereupon valve A between the two chambers is opened allowing the .chargeto pass from chamber 200 to 'hopper 200".

v' Valve A isnow closed. Discharging hopper portance of -applylinv y 200bv is now purged ofgas by'admitting steam from pipe 204 thereto through the valved connection shown, the purge passing through a A-pipe 206 to a receiver 207. ,The charge infhopper 200b from the system by'openingvalve B connected to said hopper. Previously receiving hopper 200 has been filled with fresh material, purged of air and brought up to the pressure of the system by opening valved connection 20S-leading from stove 100.

Gas and uncondensed vapors leaving condenser 202 pass back to stove 100 through a pipe 209 and pump 210. 4A relief valve 260 is provided in one of an interconnected plurality 'whereby a continuous supply of hot gasesmay be insured.'

-The foregoin system thus .provides for heat Itreating.s 'ofid carbonaceous substances by the use ofheated hydrocarbon or hydrogen containing gases. suitably controlling conditions of temperature and pressure such heat treatment may be eective to produce a simple distillation with the 'minimum vof Cracking of the libl or such heat treatment cracking ofsuch hydrocarbons. .The unheat through the medium of heated rocarbon gases is even greater when solid materials, such as shale or oil sand, are treated, than when liquid h drocarbons are being treated,l because the disadvantages and diiculties encounteredv in the directy application of heat so suchv solids 'are greater than in heat to liquids'. The conduction of heat from the wall-of avessel through crushed shale or may now be removed.

line 209. Ordinarily stove 100 is It' will be obvious that by sand, for'example, iseven poorer than the liquid. It' is 'further to be noted that the unevenness offcontact of the material to be heated with the wall introduces 'a special from such hot Wall to problem in the-.treatment of shale or sand in the other hand, since the heat If relatively high interior pres- 1 danger of overheating is applied on the same side otthe vessel walls as the lmaterial undergoing treatment.

I claim 1. In'an apparatus of the type described, a plurality of regenerative heating elements, a plurality of distillation chambers, a1 source ott heat carrier gases including a receiver,

means for admitting gases from said source to a given heating element, a gas take-off connection joining said heating elements in parallel'connecting conduits whereby the interior of anyl given distillation chamber may be operativelyconnected tol any given heating l` element, condensing means, means for joining any given distillation chamber to said condensingmeans, means orconnecting said `condensing means to 4said receiver whereby to collect the gases therefrom, means for purging each of said elements when connected to a given distillationchamber', whereby both v'said heating element and the distillation chamber connected therewith may be purged inthe same operation, and means for conducting the purgeto said receiver.

2. An apparatus' according to claim 1 in which threeheatlng elements and. three disl tillation chambers are provided thereby permlttlngthe operations of charging. distilling to take place simultaneously..

and discharging CH'ARLES. P. TOLMAN.

the direct. applicationof .1 

